Designation: C 1580 – 05
Standard Test Method for
Water-Soluble Sulfate in Soil1
This standard is issued under the fixed designation C 1580; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method is for the determination of water-
soluble sulfate in soils.
1.2 This test method was developed for concentrations of
water-soluble sulfate in soils between 0.02 and 3.33 % sulfate
by mass.
1.3 This test method does not determine sulfur in any form
except as sulfate.
1.4 Some governing bodies regulate the movement of soils
from one area to another. It is up to the sampler and laboratory
to comply with all regulations.
1.5 The values stated in SI units are to be regarded as the
standard.
1.6 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety and health practices and to determine the
applicability of regulatory limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards: 2
C 114 Test Methods for Chemical Analysis for Hydraulic
Cement
D 1193 Specification for Reagent Water
E 11 Specification for Wire and Cloth Sieves for Testing
Purposes
E 60 Practice for Analysis of Metals, Ores, and Related
Materials by Molecular Absorption Spectrometry
E 275 Practice for Describing and Measuring Performance
of Ultraviolet, Visible, and Near Infrared Spectrophotom-
eters
3. Significance and Use
3.1 This test method can be used to determine if soils could
have an adverse reaction with hydraulic cement concrete.
1
This test method is under the jurisdiction of ASTM Committee C09 on
Concrete and Aggregates and is the direct responsibility of Subcommittee on C09.69
Miscellaneous Tests.
Current edition approved March 1, 2005. Published April 2005.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
4. Apparatus
4.1 Photometer—One of the following, given in order of
preference:
4.1.1 Nephelometer or turbidimeter,
4.1.2 Spectrophotometer for use at 420 nm with light path of
4 to 5 cm, and
4.1.3 Filter photometer with a violet filter having a maxi-
mum near 420 nm and a light path of 4 to 5 cm. Filter
photometers and photometric practices prescribed in this test
method shall conform to Practice E 60; spectrophotometer
practices shall conform to Practice E 275.
4.2 Stopwatch, readable to 0.1 minutes.
4.3 Measuring Spoon, capacity 0.2 to 0.3 mL.
4.4 Drying oven, capable of continuously heating at 110 6
5º C.
4.5 Balance, shall be capable of reproducing results within
0.0002 g with an accuracy of 60.0002 g. Direct-reading
balances shall have a sensitivity not exceeding 0.0001 g.
Conventional two-pan balances shall have a maximum sensi-
bility reciprocal of 0.0003 g. Any rapid weighing device that
may be provided, such as a chain, damped motion, or heavy
riders, shall not increase the basic inaccuracy by more than
0.0001 g at any reading and with any load within the rated
capacity of the balance.
4.6 Stirrer, magnetic variable speed, with a TFE-
fluorocarbon coated magnetic stirring rod or an overhead stirrer
with a propeller.
5. Reagents and Materials
5.1 Purity of Reagents—All reagents shall conform to the
specifications of the Committee on Analytical Reagents of the
American Chemical Society.3
5.2 Purity of Water—Unless otherwise indicated, reference
to water shall be understood to mean reagent water conforming
to Specification D 1193, Type I. Other reagent water types (See
Note 1) may be used, provided it is first ascertained that the
3
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD.
 C 1580 – 05
water is of sufficiently high purity to permit its use without
adversely affecting the precision and bias of the test method.
NOTE 1—Type II water was specified at the time of round robin testing
of this test method.
5.3 Barium Chloride—Crystals of barium chloride
(BaCl2·2H2O) screened to 850 to 600 µm. To prepare in the
laboratory, spread crystals over a large watch glass, desiccate
for 24 h, screen to remove any crystals that are not 850 to 600
µm, and store in a clean, dry jar.
5.4 Conditioning Reagent—Place 30 mL of concentrated
hydrochloric acid (HCl, sp gr 1.19), 300 mL reagent water, 100
mL 95 % ethanol or isopropanol and 75 g sodium chloride
(NaCl) in a container. Add 50 mL glycerol and mix.
5.5 Sulfate Solution, Standard (1 mL = 0.100 mg SO4)—
Dissolve 0.1479 g of anhydrous sodium sulfate (Na2SO4) in
water, and dilute with water to 1 L in a volumetric flask.
5.6 pH paper, readable to at least 0.5 pH units.
5.7 Sodium Hydroxide, (0.1N)—Dissolve 4 g of sodium
hydroxide (NaOH) in water and dilute with water to 1L
5.8 Hydrochloric Acid (0.1N)—Dilute 8.6 mL of concen-
trated hydrochloric acid (HCl sp gr 1.19) to 1L with water
6. Permissible Variations
6.1 Both the referee method and qualified methods as
described in Test Methods C 114 are permissible as alternatives
to the turbidimetric procedure.
7. Calibration and Standardization
7.1 Prepare standards by diluting 0.0, 2.0, 5.0, 10.0, 15.0,
20.0, 30.0, and 40.0 mL of standard sulfate solution with water
to 100-mL volumes in volumetric flasks. These solutions will
have sulfate ion concentrations of 0.0, 2.0, 5.0, 10.0, 15.0, 20.0,
30.0, and 40.0 mg/L, respectively. Follow the procedure given
in Section 8 using appropriate amounts of the standard sulfate
solution prepared in accordance with 5.5 and prepare a
calibration curve showing sulfate ion content in mg/L plotted
against the corresponding photometer readings.
7.2 A separate calibration curve must be prepared for each
photometer and a new curve must be prepared if it is necessary
to change the cell, lamp, or filter, or if any other alterations of
instrument or reagents are made. Check the curve with each
series of tests by running two or more solutions of known
sulfate concentrations in the range of 5 to 40 mg SO4/L.
NOTE 2—The slope of the curve may not be linear below 5 or above 40
mg SO4/L for this method.
8. Procedure
8.1 Collect at least 100 g of representative soil for analysis.
Dry the sample for 18 to 24 h at 110 °C. Crush to pass a 600
µm sieve. In a 400 mL beaker labeled Sample A, put a sample
consisting of approximately 30 g. In a second 400 mL beaker
labeled Sample B, place a sample of approximately 3 g. Record
the mass of each sample to the nearest 0.001 g. Add 250 mL of
deionized water to each beaker, and stir on a magnetic stirrer
for one h. Filter the extraction through two dry medium texture
filter papers under suction. Do not wash the residue. Repeat the
filtration if solution is not clear. Check the pH of the filtrate
2
using pH paper and, if needed, neutralize each filtrate to pH of
7 6 1 using either 0.1N HCl or 0.1N NaOH.
8.2 Adjust the temperature of the solution in the volumetric
flasks to between 20 and 25 °C [68 to 77 °F].
8.3 Use an aliquot of 10 mL for specimen A1, 20 mL for
specimen A2, 10 mL for specimen B1, and 20 mL for specimen
B2. Dilute to a volume of 100 mL in a volumetric flask and
follow the procedure below or Test Methods C 114. Pour the
100 mL into a 250 mL beaker. Add 5.0 mL of conditioning
reagent. Mix by stirring with a stir bar and magnetic stirrer.
Add 0.3 g of the prepared BaCl2 crystals using a measuring
spoon and start the timer.
8.4 Stir exactly 1.0 min, at the same constant speed for all
determinations.
8.5 Remove the beaker from the stirrer, pour solution into
the cell, and put the cell into the photometer. Record the
turbidity at 4.0 min after pouring the solution into the cell.
8.6 Determine the mg of SO4 from the calibration curve.
9. Calculation or Interpretation of Results
9.1 Calculate the sulfate content (% by mass) for each
specimen as follows:
·
2.5*M
P 5 A*W (1)
Where:
P = % SO4 in dried soil
M = mg/L of SO4 calculated from calibration curve
W = mass of soil placed into 400 mL beaker, in g
A = volume of aliquot specimen, in mL
9.2 Limits of values for results to be valid. (See Note 3)
Specimen Lower Limit Upper Limit
A1 0.04% 0.33%
A2 0.02% 0.17%
B1 0.41% 3.33%
B2 0.21% 1.67%
1. Determine which results fall within the above limits
2. Discard those that do not
3. Average all results that comply
NOTE 3—These values were derived from the limits on the sulfate test
of 5 to 40 mg/L, and a solubility of sulfate of 1.6 g/L at pH 7 when calcium
sulfate is present. The method is not applicable for soils outside this range.
For those samples, see the Annex.
10. Report
10.1 Report the average obtained as % sulfate by mass of
sample. If milligrams sulfate in kilograms of soil (mg SO4/kg
soil) is desired, multiply % sulfate by 10 000. Report results to
nearest 0.01 % or 100 mg/kg.
11. Precision and Bias
11.1 Precision—The standard deviation was found to vary
with concentration, so therefore, a coefficient of variation was
used for the precision statement. The single operator coefficient
of variation was found to be 4.4 %. Therefore, results of two
properly conducted tests by the same operator on the same
material should not differ by more than 12.4 % of their
average. The multilaboratory coefficient of variation was found
to be 21.2 %. Therefore, results of two different laboratories on
 C 1580 – 05
identical samples of a material should not differ from each 12. Keywords
other by more than 60 % of their average.
12.1 hydraulic cement; soil; Sulfate; turbidimeter
11.2 Bias—Since there is no accepted reference material
suitable for determining bias, bias can not be determined.

ANNEX

(Mandatory Information)

A1. REDUCING THE NUMBER OF SUB-SAMPLES AND SAMPLES OUT OF COMPLIANCE

A1.1 This procedure was written to accommodate labora-
tories that are not familiar with the soil under test. If prior
knowledge is available, a lesser number of sub-samples, and/or
dilutions may be used.
A1.2 If a sample falls above 3.33 % sulfate, then different
sample masses and/or dilutions can be used. If this procedure
is followed, then the mg SO4 from the turbidimeter reading
shall be maintained within 5 to 40 mg/L. If another procedure
is used, then validation shall be provided showing that the
results are within the linear range of the calibration.

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